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A kind of preparation method of green chelating agent

A chelating agent and catalyst technology, applied in the field of organic synthesis catalysis, can solve the problems of easily corroded production equipment, high impurity content in products, difficult biodegradation, etc. degree of effect

Active Publication Date: 2022-01-04
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

4A zeolite is generally used to replace phosphate in washing powder. In the process of activated sludge treatment of wastewater, phosphonate is easily adsorbed on the surface of activated sludge, but it is difficult to biodegrade
Patent CN101784513B introduces a method for preparing glutamic acid-N,N-diacetic acid alkali metal salts using L-glutamic acid, formaldehyde and hydrogen cyanide and its salts as raw materials. The product of this method has high impurity content, and The raw material hydrocyanic acid used is highly toxic, and the waste water produced contains a large amount of cyanide residue, and it is easy to corrode the production equipment
Chinese patent 201210073918.X discloses a method of using zinc salt to catalyze the reaction of L-glutamic acid and 2-chloroacetonitrile in an organic base system such as pyridine and triethylamine, and then neutralizing the base with sodium hydroxide to prepare glutamic acid Tetrasodium diacetate (GLDA.Na 4 ), because the solubility of L-glutamic acid in water at room temperature is extremely low, so this method needs to dissolve glutamic acid at high temperature and then lower it to low temperature to add raw materials 2-chloroacetonitrile and organic base. After alkali, it needs to reflux to discharge the generated ammonia, and the generated product has a dark color. This method has complicated process operation, long process cycle and high energy consumption.
It is reported in Chinese literature that L-glutamic acid and chloroacetic acid are used as raw materials, LiOH is added to adjust the pH of the system and mixed uniformly, heated for 5 to 6 hours, acidified with hydrochloric acid, recrystallized and washed with decompressed ethanol to prepare N , the method of N-dicarboxymethyl-L-glutamic acid, the yield of the product prepared by this method is low, the reaction time is long, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) At room temperature, respectively add 285g of sodium glutamate monohydrate, 153g of 32% aqueous sodium hydroxide solution by mass, 110g of deionized water and 0.5g of KI into the reaction kettle in sequence, stir and mix evenly;

[0029] (2) Dissolve 310g of chloroacetic acid in 217g of deionized water and put it into a constant pressure dropping funnel for later use;

[0030] (3) Feed nitrogen into the reactor for 10-15min, after stopping, put 544g of 50% sodium hydroxide aqueous solution into another constant pressure dropping funnel for subsequent use;

[0031] (4) Raise the temperature of the reactor system to 80°C, add the aqueous solution of chloroacetic acid in step (2) and the liquid caustic soda in step (3) dropwise, and control the dropping rate to keep the pH value of the reaction system in the range of 10~10.5 ;

[0032] (5) After 3 hours of dropwise addition, keep warm at 85±2°C for 1 hour;

[0033] (6) After the heat preservation is completed, filter...

Embodiment 2

[0036] (1) At room temperature, respectively add 180g of L-alanine, 200g of 32% aqueous sodium hydroxide solution by mass, 42g of deionized water and 0.5g of KI into the reaction kettle in sequence, stir and mix evenly;

[0037] (2) Dissolve 420g of chloroacetic acid in 300g of deionized water, and put it into a constant pressure dropping funnel for later use;

[0038] (3) Feed nitrogen into the reaction kettle for 10-15min, after stopping, put 765g of 50% sodium hydroxide aqueous solution into another constant pressure dropping funnel for standby;

[0039] (4) Raise the temperature of the reactor system to 80°C, add the aqueous solution of chloroacetic acid in step (2) and the liquid caustic soda in step (3) dropwise, and control the dropping rate to keep the pH value of the reaction system in the range of 10~10.5 ;

[0040] (5) After 3.5 hours of dropping, keep warm at 85±2°C for 1 hour;

[0041] (6) After the heat preservation is over, filter while it is hot, and dilute t...

Embodiment 3

[0043](1) At room temperature, respectively add 120g of L-aspartic acid, 100g of 32% aqueous sodium hydroxide solution by mass, 30g of deionized water and 0.36g of NaI into the reaction kettle in sequence, stir and mix evenly;

[0044] (2) Dissolve 215g of chloroacetic acid in 154g of deionized water, and put it into a constant pressure dropping funnel for later use;

[0045] (3) Feed nitrogen into the reaction kettle for 10-15min, after stopping, put 212g of 50% sodium hydroxide aqueous solution into another constant pressure dropping funnel for standby;

[0046] (4) Raise the temperature of the reactor system to 80°C, add the aqueous solution of chloroacetic acid in step (2) and the liquid caustic soda in step (3) dropwise, and control the dropping rate to keep the pH value of the reaction system in the range of 10~10.5 ;

[0047] (5) After 2 hours of dropping, keep warm at 85±2°C for 0.5 hours;

[0048] (5) After the heat preservation is over, filter while it is hot, and ...

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Abstract

The invention provides a preparation method of a green chelating agent. Specifically, under normal pressure conditions, the use of partially neutralized amino acids and chloroacetic acid produces S under the action of a catalyst. N 2 Bimolecular nucleophilic substitution reaction to prepare a series of green chelating agents, wherein the catalyst is iodide of alkali metal, and the amount of catalyst used is 0.01-0.30% of the input mass of amino acid. The method of the present invention adopts an atmospheric pressure catalytic reaction system, the catalyst usage is small, and the treatment method is simple; the catalytic performance is good, and the product yield can reach more than 96%; Chemical industry production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis catalysis and provides a preparation method for synthesizing a green chelating agent by using alkali metal iodide to catalyze amino acid and chloroacetic acid as raw materials. Background technique [0002] Ethylenediaminetetraacetic acid (EDTA), aminotriacetic acid (NTA), sodium tripolyphosphate (STPP), etc. are widely used in various washing formulas as chelating additives. However, NTA has recently been listed as a potential carcinogen, EDTA Poor biodegradability, STPP will lead to eutrophication of rivers and lakes. With the increasing awareness of people's health and environmental protection and the stricter regulations, these traditional detergents will be replaced by green chelating agents. Following the trend of greening chelating agents, many chemical manufacturers have launched various green alternatives. Ideal green alternatives should have excellent cost performance, be pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/18C07C229/24C07C229/16
CPCC07C227/18C07C229/24C07C229/16
Inventor 陈树招赵坤王宁宁周响刘全华陆久田张敏
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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